US8685290B2 - Glass-crystalline particle powders including a glass component and a crystalline component - Google Patents
Glass-crystalline particle powders including a glass component and a crystalline component Download PDFInfo
- Publication number
- US8685290B2 US8685290B2 US12/891,218 US89121810A US8685290B2 US 8685290 B2 US8685290 B2 US 8685290B2 US 89121810 A US89121810 A US 89121810A US 8685290 B2 US8685290 B2 US 8685290B2
- Authority
- US
- United States
- Prior art keywords
- glass
- crystalline
- component
- particles
- composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related, expires
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- 239000011521 glass Substances 0.000 title claims abstract description 138
- 239000002245 particle Substances 0.000 title claims abstract description 137
- 239000000843 powder Substances 0.000 title claims description 49
- 239000000203 mixture Substances 0.000 claims abstract description 92
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 35
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 12
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 10
- 229910052788 barium Inorganic materials 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 9
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 9
- 238000010304 firing Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 34
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 32
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 26
- 239000011701 zinc Substances 0.000 description 25
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 24
- 238000000034 method Methods 0.000 description 23
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 22
- 239000000443 aerosol Substances 0.000 description 22
- 239000002243 precursor Substances 0.000 description 19
- 238000002441 X-ray diffraction Methods 0.000 description 17
- 239000000377 silicon dioxide Substances 0.000 description 16
- 229910052681 coesite Inorganic materials 0.000 description 15
- 229910052906 cristobalite Inorganic materials 0.000 description 15
- 229910052682 stishovite Inorganic materials 0.000 description 15
- 229910052905 tridymite Inorganic materials 0.000 description 15
- 238000009826 distribution Methods 0.000 description 14
- 229910011255 B2O3 Inorganic materials 0.000 description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- 229910052593 corundum Inorganic materials 0.000 description 13
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 13
- 229910001845 yogo sapphire Inorganic materials 0.000 description 13
- 238000001878 scanning electron micrograph Methods 0.000 description 12
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 11
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 11
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 11
- 239000002904 solvent Substances 0.000 description 11
- 229910052844 willemite Inorganic materials 0.000 description 11
- 239000011787 zinc oxide Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 10
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 8
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000000470 constituent Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000012159 carrier gas Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 230000000704 physical effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229910002651 NO3 Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000006060 molten glass Substances 0.000 description 6
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 229910052797 bismuth Inorganic materials 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 239000004110 Zinc silicate Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 4
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 4
- 235000019352 zinc silicate Nutrition 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 238000004581 coalescence Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 3
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- -1 Bi(OH)3 Chemical compound 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000001856 aerosol method Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 238000005136 cathodoluminescence Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000004031 devitrification Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- FPHIOHCCQGUGKU-UHFFFAOYSA-L difluorolead Chemical compound F[Pb]F FPHIOHCCQGUGKU-UHFFFAOYSA-L 0.000 description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000000804 electron spin resonance spectroscopy Methods 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000005816 glass manufacturing process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N lead(II) oxide Inorganic materials [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Inorganic materials [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000004846 x-ray emission Methods 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 1
- RUJPNZNXGCHGID-UHFFFAOYSA-N (Z)-beta-Terpineol Natural products CC(=C)C1CCC(C)(O)CC1 RUJPNZNXGCHGID-UHFFFAOYSA-N 0.000 description 1
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- KOPBYBDAPCDYFK-UHFFFAOYSA-N Cs2O Inorganic materials [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229920000896 Ethulose Polymers 0.000 description 1
- 239000001859 Ethyl hydroxyethyl cellulose Substances 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000004813 Moessbauer spectroscopy Methods 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Inorganic materials [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 1
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Inorganic materials [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium nitrate Inorganic materials [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 229960002380 dibutyl phthalate Drugs 0.000 description 1
- AKUNKIJLSDQFLS-UHFFFAOYSA-M dicesium;hydroxide Chemical compound [OH-].[Cs+].[Cs+] AKUNKIJLSDQFLS-UHFFFAOYSA-M 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019326 ethyl hydroxyethyl cellulose Nutrition 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910052839 forsterite Inorganic materials 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(II) nitrate Inorganic materials [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- NOTVAPJNGZMVSD-UHFFFAOYSA-N potassium monoxide Inorganic materials [K]O[K] NOTVAPJNGZMVSD-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001812 pycnometry Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- AHLATJUETSFVIM-UHFFFAOYSA-M rubidium fluoride Inorganic materials [F-].[Rb+] AHLATJUETSFVIM-UHFFFAOYSA-M 0.000 description 1
- 229910001953 rubidium(I) oxide Inorganic materials 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Inorganic materials [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 1
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Images
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- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
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- C03C3/00—Glass compositions
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Definitions
- the invention relates to glass-crystalline particle powders including a glass component and a crystalline component.
- Glass powder applications require glass powders that have one or more of the following properties: high purity, controlled chemistry, spherical morphology, small average size, narrow size distribution, and little or no agglomeration.
- Glass powder applications requiring such characteristics include, but are not limited to, thick film pastes used for fabricating electronic devices. Thick film pastes are mixture of the powders in an organic vehicle, wherein the organic vehicle is removed after application of the paste to a substrate by firing the composition at elevated temperatures.
- glass powders are produced by forming a melt of the desired glass composition, quenching the molten glass and milling the resulting glass to reduce the particle size.
- a glass lacks the long range regular periodic arrangement of atoms characteristic of materials considered crystalline to one skilled in the art.
- the resulting data lacks the distinct peaks seen in materials considered crystalline, yet instead shows a broad signal over wider range of 2 ⁇ angles; this range being typical greater than 5 to 20° 2 ⁇ .
- the milling process results in glass powders having an irregular morphology and high surface area which can be undesirable in precision applications.
- Aerosol decomposition of an atomized liquid spray of precursor solution is a useful method for producing glass-crystalline particles and spherical glass-crystalline particles with high purity, controlled chemistry, small average size, narrow size distribution, and little or no agglomeration.
- a precursor solution containing the elements desired in the final glass is atomized to produce an aerosol.
- the aerosol particles are then transported through a reaction tube where the solvent is removed and the aerosol particles are heated to a temperature sufficiently high to convert the precursor compounds to product glass particles. At these high temperatures a suitable material of construction reactor tube needs to be used.
- the invention relates to a plurality of glass-crystalline particles, wherein at least a portion of the glass-crystalline particles include a glass component and a crystalline component, and wherein the crystalline component includes one or more metal oxides wherein the metal is selected from the group consisting of: Zn, Ca, Sr, Mg, Ba, and mixtures thereof. At least a portion of the glass-crystalline particles may be substantially spherical.
- An aspect relates to a powder including the plurality of glass-crystalline particles.
- the surface area of at least a portion of the particles may be between 0.1 m 2 /g and 3.0 m 2 /g.
- the d 50 may be between 0.2 microns and 3.0 microns.
- the d 95 may be between 0.5 microns and 5.0 microns.
- the surface area divided by the d 10 of at least a portion of the glass-crystalline particles may be between 0.5 m 2 /g ⁇ m and 5.0 m 2 /g ⁇ m.
- the surface area divided by the d 50 of at least a portion of the glass-crystalline particles may be between 0.3 m 2 /g ⁇ m and 3.0 m 2 /g ⁇ m.
- the surface area divided by the d 95 of at least a portion of the glass-crystalline particles may be between 0.2 m 2 /g ⁇ m and 2.0 m 2 /g ⁇ m.
- An embodiment relates to a plurality of glass-crystalline particles, wherein at least a portion of the glass-crystalline particles may be spherical, wherein at least a portion of the glass-crystalline particles may include a glass component and a crystalline component, and wherein the crystalline component may include one or more metal oxides.
- the metal of the one or more metal oxides may be selected from the group consisting of: Zn, Ca, Sr, Mg, Ba, and mixtures thereof.
- the surface area may be from 0.1 m 2 /g to 3.0 m 2 /g.
- An embodiment relates to a plurality of glass-crystalline particles, wherein at least a portion of the glass-crystalline particles include a glass component and a crystalline component, wherein the crystalline component may be 45-80 wt % of the particle, and wherein the crystalline component may include one or more metal oxides.
- An aspect relates to a thick film composition including an organic medium, a conductive powder, and a plurality of glass-crystalline particles.
- a further aspect relates to a device including, prior to firing, a thick film composition.
- FIG. 1A shows the BS-SEM picture of Example 1 showing the spherical glass-crystalline particles.
- the lighter areas are the glass component, and the darker areas are the crystalline components containing zinc oxide.
- FIG. 1B shows the BS-SEM picture of Comparative example 1 in which the glass particles are the light colored particles and the dark areas are zinc silicate.
- FIG. 1C illustrates the surface of a spherical glass-crystalline particle containing a low % of crystalline metal oxide.
- the white areas represent glass components and the dark areas represent crystalline components.
- FIG. 1D illustrates the surface of a spherical glass-crystalline particle with more crystalline metal oxide.
- the white areas represent glass components and the dark areas represent crystalline components.
- FIG. 2A shows the XRD (X-ray Diffraction) pattern of the spherical glass-crystalline particles of Example 1 showing the amorphous glass pattern (very broad peak) and the crystalline peaks of zinc oxide and zinc silicate.
- FIG. 2B is the XRD pattern from the glass particles and zinc silicate particles from Comparative example 1, showing the amorphous glass pattern evident by the broad signal over the range 20°-40° 2 ⁇ and the crystalline peaks of zinc silicate only, and no peak corresponding to zinc oxide.
- An aspect of the invention relates to a glass-crystalline particle including a glass component and a crystalline component wherein the crystalline component includes one or more metal oxides and the method of making the glass-crystalline particles.
- the metal in the metal oxides may be one or more metal oxides selected from the group consisting of Zn, Mg, Ca, Sr, Ba, and mixtures thereof.
- a further aspect of the invention relates to a glass-crystalline particle including a composition that contains a glass component and a crystalline component wherein the crystalline component is between 45 wt % and 80 wt %, based on the weight of the composition.
- the crystalline composition may be 45 wt % to 72 wt %, based on the weight of the composition.
- the crystalline composition may be between 50 wt % to 68 wt %, based on the weight of the composition.
- a portion of the crystalline component may be on the surface of the particle. In an embodiment, 5% to 100% of the crystalline component may be on the surface of the particle.
- a further aspect of the invention relates to a glass-crystalline particle including a composition that contains a glass component and a crystalline component wherein the glass component is between 20 wt % to 55 wt %, based on the weight of the composition.
- the glass composition may be between 28 wt % to 55 wt %, based on the weight of the composition.
- the glass composition may be between 32 wt % and 50 wt %, based on the weight of the composition.
- the glass-crystalline particle may have areas on the surface that are crystalline metal oxide and separate areas on the surface that are glass.
- FIG. 1 shows the BS-SEM picture presenting the areas on the surface that are glass and other areas on the surface that are the crystalline metal oxide.
- the crystalline component may include distinct separate crystals.
- the crystals may include a metal oxide.
- the crystals may also include a metal silicate.
- the crystals may be the same shape, or different shapes.
- the crystals may be rectangular, hexagons, ovals, for example.
- An aspect of the invention relates to a glass-crystalline powder containing a plurality of glass-crystalline particles including a glass component and a crystalline component wherein the crystalline component includes one or more crystalline metal oxides and the method for making glass-crystalline powders.
- the metal in the metal oxides may be one or more metal oxides selected from the group consisting of Zn, Mg, Ca, Sr, Ba, and mixtures thereof.
- the metal in the metal oxide may be Zn, Mg, or mixtures thereof.
- the metal in the metal oxide may be Zn.
- the glass-crystalline particle may be spherical in shape.
- the surface area to particle size ratio is minimized, as compared to non-spherical particles.
- a further aspect of the invention relates to a spherical glass-crystalline particle including a glass component and a crystalline component wherein the crystalline component includes one or more metal oxides and the method for producing spherical glass-crystalline particles.
- the metal in the metal oxides is one or more metal oxides selected from the group consisting of Zn, Mg, Ca, Sr, Ba, and mixtures thereof.
- a further aspect of the invention relates to a spherical glass-crystalline particle including a composition that contains a glass component and a crystalline component wherein the crystalline component may be between 45 wt % and 80 wt %, based on the weight of the composition.
- the crystalline composition may be between 45 wt % and 72 wt %, based on the weight of the composition.
- the crystalline composition may be between 50 wt % and 68 wt %, based on the weight of the composition.
- a portion of the crystalline component may be on the surface of the particle.
- a further aspect of the invention relates to a spherical glass-crystalline particle including a composition that contains a glass component and a crystalline component wherein the glass component may be between 20 wt % and 55 wt %, based on the weight of the composition.
- the crystalline composition may be between 28 wt % and 55 wt %, based on the weight of the composition.
- the crystalline composition may be between 32 wt % and 50 wt %, based on the weight of the composition.
- a further aspect of the invention relates to a spherical glass-crystalline powder containing a plurality of spherical glass-crystalline particles including a glass component and a crystalline component wherein the crystalline component includes one or more crystalline metal oxides and the method to prepare spherical glass-crystalline powders.
- the metal in the metal oxides may be one or more metal oxides selected from the group consisting of Zn, Mg, Ca, Sr, Ba, and mixtures thereof.
- the glass-crystalline powder or spherical glass-crystalline powder may have a low surface area.
- the surface area ranges from 0.1 m 2 /g to 3.0 m 2 /g.
- the surface area ranges from 0.5 m 2 /g to 3.0 m 2 /g.
- the surface area ranges from 0.5 m 2 /g to 2.0 m 2 /g.
- the spherical glass-crystalline powder may be small in size with a particle size distribution.
- the particle size distribution is characterized by specific percent volume distribution sets; d 10 refers to the 10% volume distribution set; d 50 refers to the 50% volume distribution set; and d 95 refers to the 95% volume distribution set.
- the glass-crystalline powders or spherical glass-crystalline powders may have d 50 from 0.2 microns to 3.0 microns, and d 95 is from 0.5 to 5.0 microns.
- the d 50 may be from 0.5 microns to 3.0 microns and the d 95 may be from 1.0 microns to 5.0 microns.
- the d 50 may be from 0.7 microns to 2.0 microns and d 95 from 1.0 microns to 4.0 microns.
- the spherical glass-crystalline powder may have a small ratio of surface to particle size distribution.
- the surface area divided by the d 10 may be from 0.5 m 2 /g ⁇ m to 5.0 m 2 /g ⁇ m
- the surface area divided by the d 50 may be from 0.3 m 2 /g ⁇ m to 3.0 m 2 /g ⁇ m
- the surface area divided by the d 95 may be from 0.2 to m 2 /g ⁇ m 2.0 m 2 /g ⁇ m.
- the surface area divided by the d 10 may be from 1.0 m 2 /g ⁇ m to 5.0 m 2 /g ⁇ m
- the surface area divided by the d 50 may be from 0.5 m 2 /g ⁇ m to 3.0 m 2 /g ⁇ m
- the surface area divided by the d 95 may be from 0.2 m 2 /g ⁇ m to 1.5 m 2 /g ⁇ m.
- the surface area divided by the d 10 may be from 1.0 m 2 /g ⁇ m to 4.0 m 2 /g ⁇ m
- the surface area divided by the d 50 may be from 0.5 m 2 /g ⁇ m to 2.0 m 2 /g ⁇ m
- the surface area divided by the d 95 may be from 0.3 m 2 /g ⁇ m to 1.0 m 2 /g ⁇ m.
- a further aspect of the invention relates to a method for the manufacture of glass-crystalline particles or spherical glass-crystalline particles including a glass component and a crystalline component wherein the crystalline component includes one or more crystalline metal oxide components including metal oxides including the sequential steps:
- precursor solution means the solution containing the solvent and the glass component composition and the crystalline component composition.
- glass component compositions are listed in Table 1 below.
- Glass component compositions are described herein as including percentages of certain glass component composition constituents. Specifically, the percentages are the percentages of oxide or fluoride components that one skilled in the art of glass making or inorganic chemistry would expect to result from the processing as described herein to form the glass component composition. Such nomenclature is conventional to one of skill in the art. In other words, the glass component composition contains certain constituents, and the percentages of those constituents are expressed as a percentage of the corresponding oxide form.
- one of skill in the art may calculate the percentages of starting glass component composition constituents described herein using methods known to one of skill in the art including, but not limited to: Inductively Coupled Plasma-Emission Spectroscopy (ICPES), Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES), and the like.
- ICPES Inductively Coupled Plasma-Emission Spectroscopy
- ICP-AES Inductively Coupled Plasma-Atomic Emission Spectroscopy
- XRF X-Ray Fluorescence spectroscopy
- NMR Nuclear Magnetic Resonance spectroscopy
- EPR Electron Paramagnetic Resonance spectroscopy
- Mössbauer Mössbauer spectroscopy
- EDS Electron microprobe Energy Dispersive Spectroscopy
- WDS Electron microprobe Wavelength Dispersive Spectroscopy
- CL Cathodoluminescence
- the glass component composition may include one or more glass former constituents.
- the glass component of the glass-crystalline particle may include one or more glass former constituents.
- Glass former constituents may include, but are not limited to: SiO 2 , P 2 O 5 , B 2 O 3 , and GeO 2 .
- the one or more glass former constituents may be 1 to 90 wt %, 2 to 60 wt %, or 3 to 55 wt % of the glass component composition.
- glass component compositions described herein including those listed in Table I, are not limiting; it is contemplated that one of ordinary skill in the art of glass chemistry could make minor substitutions of additional ingredients and not substantially change the desired properties of the glass component composition.
- substitutions of glass formers such as P 2 O 5 0-3, GeO 2 0-3, V 2 O 5 0-3 in weight % may be used either individually or in combination to achieve similar performance.
- one or more intermediate oxides such as TiO 2 , Ta 2 O 5 , Nb 2 O 5 , ZrO 2 , CeO 2 , and SnO2 may be substituted for other intermediate oxides (i.e., Al 2 O 3 , CeO 2 , SnO 2 ) present in a glass component composition.
- glass component compositions described herein in weight percent total glass component composition, are shown in Table 1.
- glass component compositions described herein may include one or more of SiO 2 , Al 2 O 3 , PbO, ZrO 2 , B 2 O 3 , Na 2 O, Li 2 O, Bi 2 O 3 , CeO 2 , TiO 2 , or anionic fluorine.
- SiO 2 may be 10 to 40 wt %, 12 to 35 wt %, or 17 to 25 wt %
- Al 2 O 3 may be 0 to 1 wt %, 0.25 to 0.35 or 0.35 to 0.45 wt %, wt %
- ZrO 2 may be 0 to 6 wt %, 0.1 to 5 wt %, or 4 to 5 wt %
- PbO may be 0 to 65 wt %, 45 to 65 wt %, or 50 to 55 wt %
- B 2 O 3 may be 1 to 10 wt %, 5 to 9 wt %, or 3 to 5 wt %
- TiO 2 may be 0 to 7 wt %, 4.5 to 6.5 wt %, or 1.5 to 2.5 wt %
- Na 2 O may be 0 to 7 wt %, 0.1 to 5 wt %, or 1 to 3 wt %
- glass component compositions described herein may include one or more of SiO 2 , Al 2 O 3 , ZrO 2 , B 2 O 3 , Na 2 O, Li 2 O, Bi 2 O 3 , CeO 2 , and TiO2.
- SiO 2 SiO 2
- Al 2 O 3 ZrO 2
- B 2 O 3 Na 2 O
- Li 2 O Li 2 O
- Bi 2 O 3 CeO 2
- TiO2 TiO2
- SiO 2 may be 10 to 35 wt %, 15 to 30 wt %, or 20 to 25 wt %
- Al 2 O 3 may be 0 to 1 wt %, 0.1 to 0.35 wt %, or 0.25 to 0.3 wt %
- ZrO 2 may be 0 to 6 wt %, 0.1 to 5 wt %, or 4 to 5 wt %
- B 2 O 3 may be 1 to 5 wt %, 3 to 5 wt %, or 3.75 to 4.25 wt %
- TiO 2 may be 0 to 3 wt %, 1 to 2.5 wt %, or 1.75 to 2.25 wt %
- Na 2 O may be 0 to 7 wt %, 0.1 to 5 wt %, or 1 to 3 wt %
- Li 2 O may be 0 to 7 wt %, 0.1 to 5 wt %, or 1 to 3 wt
- glass component compositions described herein may include one or more of SiO 2 , Al 2 O 3 , PbO, B 2 O 3 , Bi 2 O 3 , TiO 2 , or anionic fluorine.
- SiO 2 may be 10 to 40 wt %, 12 to 25 wt %, or 17 to 23 wt %
- Al 2 O 3 may be 0 to 1 wt %, 0.1 to 0.5 wt %, or 0.35 to 0.45 wt %
- PbO may be 40 to 70 wt %, 45 to 65 wt %, or 50 to 60 wt %
- B 2 O 3 may be 5 to 10 wt %, 6 to 9 wt %, or 6.5 to 8 wt %
- TiO 2 may be 3 to 7 wt %, 4.5 to 6.5 wt %, or 5 to 6 wt %
- Bi 2 O 3 may be 1 to 10 wt %, 5 to 8 wt %, or 6 to 7 wt %
- F may be 1 to 7 wt %, 4 to 7 wt %, or 1 to 2 wt %, based on the weight of the glass
- One skilled the art of making glass could replace some or all of the F, Na 2 O or Li 2 O with NaF, LiF, KF, CsF, RbF, K 2 O, Cs 2 O, or Rb 2 O and create a glass component with properties similar to the compositions listed above where this embodiment the total alkali metal oxide or metal fluoride content may be 0 to 7 wt %, 0.1 to 5 wt %, or 1 to 3 wt %, based on the weight of the glass component composition.
- the glass component composition(s) herein may include one or more of a third set of components: CeO 2 , SnO 2 , Ga 2 O 3 , In 2 O 3 , NiO, MoO 3 , WO 3 , Y 2 O 3 , La 2 O 3 , Nd 2 O 3 , FeO, HfO 2 , Cr 2 O 3 , CdO, Nb 2 O 5 , Ag 2 O, Sb 2 O 3 , and metal halides (e.g. NaCl, KBr, NaI).
- a third set of components CeO 2 , SnO 2 , Ga 2 O 3 , In 2 O 3 , NiO, MoO 3 , WO 3 , Y 2 O 3 , La 2 O 3 , Nd 2 O 3 , FeO, HfO 2 , Cr 2 O 3 , CdO, Nb 2 O 5 , Ag 2 O, Sb 2 O 3 , and metal halides (e.g. NaCl, KBr
- the choice of raw materials could unintentionally include impurities that may be incorporated into the glass component during processing.
- the impurities may be present in the range of hundreds to thousands ppm. The presence of the impurities would not alter the properties of the glass component.
- Any soluble salt can be used in the method of the invention in the glass precursor solution used to form the aerosols.
- Examples include metal nitrates, fluorides, chlorides, phosphates, sulfates, acetates, and the like.
- Specific examples include the suitable salts: Al(NO 3 ) 3-9 H 2 O, Bi(NO 3 ) 3 , H 3 BO 3 , Bi(OH) 3 , LiNO 3 , Zr(NO 3 ) 4 , Zn(NO 3 ) 2 , NaNO 3 , NaF, Pb(NO 3 ) 2 , PbF 2 , Mn(CH 3 COO) 2 , Mn(NO 3 ) 2 , and the like.
- These soluble salts may be used in concentrations to just below the solubility limit of the particular salt.
- the total glass component and crystalline component may be from 0.5 wt % to 20 wt %, based on the weight of the precursor solution. In a further embodiment, the total glass component and crystalline component may be from 1.0 wt % to 10 wt %, based on the weight of the precursor solution.
- water-soluble salts may be used as the source for the glass-crystalline particle components or spherical glass-crystalline particle components
- solvent-soluble components such as organometallic compounds dissolved in either aqueous, organic solvents, or inorganic solvents.
- Colloidal particles (smaller than 100 nanometers in size) containing compounds or elements may also be used for the glass-crystalline particle components or spherical glass-crystalline particle components provided the colloidal particles form a stable suspension in the precursor solution.
- any of the conventional apparatus for droplet generation may be used to prepare the aerosols for the invention including, but not limited to, nebulizers, Collison nebulizers, ultrasonic nebulizers, vibrating orifice aerosol generators, centrifugal atomizers, two-fluid atomizers, electrospray atomizers and the like.
- the particle size distribution of the glass powder is a direct function of the distribution of droplet sizes generated.
- the size of the droplets in the aerosol is not critical in the practice of the method of the invention. However, as mentioned above, it is important that the number of droplets not be so great as to incur excessive coalescence which broadens the particle size distribution.
- concentration of the solution of the precursor components has an effect on particle size.
- particle size is an approximate function of the cube root of the concentration. Therefore, the higher the precursors component's concentration, the larger the particle size of the spherical glass particle. If a greater change in particle size is needed, a different aerosol generator may be used.
- any gas which is inert or oxidizing can be used for the carrier gas and/or the quench gas.
- suitable inert gases include nitrogen and argon and suitable oxidizing gases include air, ozone, or nitrogen dioxide.
- air may be used for the carrier gas and quench gas since it is oxidizing and is low cost.
- the temperature range over which the method of the invention can be carried out is quite wide and ranges from the reaction temperature of the glass-crystalline particle components to the crystallization temperature of the glass component.
- This reaction temperature range varies from 300° C. to 1500° C. It is important to operate at a high enough temperature for the spherical glass-crystalline particle glass components and the crystalline components to react. In an embodiment, the reaction temperature may be above 600° C. to ensure complete reaction of the particles.
- the type of apparatus used to heat the aerosol is not by itself critical and either direct or indirect heating may be used.
- tube furnaces may be used or direct heating in combustion flames may be used. It is important to control the temperature so that the glass-crystalline particle components crystallize to form the glass-crystalline particle comprising a glass component and a crystalline component wherein the crystalline component comprises one or more metal oxides.
- the glass-crystalline components or spherical glass-crystalline components Upon reaching the reaction temperature and the glass-crystalline components or spherical glass-crystalline components are reacted, they are separated from the carrier gas, reaction by-products, and solvent volatilization products and the spherical glass-crystalline powder collected by one or more devices such as filters, cyclones, electrostatic separators, bag filters, filter discs and the like.
- the gas Upon completion of the reaction, the gas consists of the carrier gas, volatile decomposition products of the spherical glass-crystalline particle components and solvent vapor.
- the effluent gas from the method of the invention will consist of nitrogen oxides, water, oxygen gas, nitrogen gas, and carbon dioxide gas.
- An embodiment relates to thick film compositions, also termed thick film pastes including the glass-crystalline powders or the spherical glass-crystalline powders described herein, conductive metal particles, and an organic medium.
- the thick film compositions may have suitable consistency and rheology for printing.
- the conductive metal particles may be powders or flakes.
- the conductive metal particles may be one or more of the following: Ag, Pt, Pd, Cu, Au, and Al.
- the organic medium is a fugitive material, in that it is burnt off during the firing process. A wide variety of inert viscous materials can be used as organic medium.
- the organic medium must be one in which the metal powders are dispersible with an adequate degree of stability.
- the rheological properties of the medium must be such that they lend good application properties to the composition, including: stable dispersion of metal powders, appropriate viscosity and thixotropy for applying the material to a substrate, appropriate paste wettability of the substrate, and a good drying rate.
- the methods for applying the materials to the substrate include, but are not limited to: screen printing, extrusion, tape casting, dip coating, spray coating, and ink jetting.
- the organic vehicle used in the thick film composition of the present invention is preferably a non-aqueous inert liquid. Use can be made of any of various organic vehicles, which may or may not contain thickeners, stabilizers and/or other common additives.
- the organic medium is typically a solution of polymer(s) in solvent(s).
- a small amount of additives may be a part of the organic medium.
- the most frequently used polymer for this purpose is ethyl cellulose.
- Other examples of polymers include ethylhydroxyethyl cellulose, wood rosin, mixtures of ethyl cellulose and phenolic resins, polymethacrylates of lower alcohols, and monobutyl ether of ethylene glycol monoacetate can also be used.
- solvents found in thick film compositions are ester alcohols and terpenes such as alpha- or beta-terpineol or mixtures thereof with other solvents such as kerosene, dibutylphthalate, butyl carbitol, butyl carbitol acetate, hexylene glycol and high boiling alcohols and alcohol esters.
- volatile liquids for promoting rapid hardening after application on the substrate can be included in the vehicle.
- Various combinations of these and other solvents are formulated to obtain the viscosity and volatility requirements desired.
- the polymer present in the organic medium may be in the range of 1 wt % to 11 wt % of the total organic composition.
- the thick film composition of the present invention may be adjusted to a predetermined, screen-printable viscosity with the organic medium.
- the ratio of organic medium in the thick film composition to the metal and inorganic components is dependent on the method of applying the paste and the kind of organic medium used, and it can vary.
- the dispersion may contain 70-95 wt % of metal and inorganic components and 5-30 wt % of organic medium (vehicle) in order to obtain good wetting.
- Table 2 describes the components of the precursor solutions for the Examples, made according the methods described in the Examples.
- Table 3 describes the physical properties of the materials described in the Examples.
- the tap density was measured using a tap density machine manufactured by Englesmann.
- the surface area was measured using a Micromeritics Tristar using the BET method.
- the He pycnometry density was measured using a Micromeritics Accupyc 1330.
- X-ray diffraction (XRD) was measured using a Rigaku Miniflex x-ray diffractometer for identification of the specific crystalline metal oxides which the glass-crystalline powders comprise.
- the particle size data was measured using a Micromeritics S3500.
- SEM Scanning electron micrographs
- BS-SEM back scatter scanning electron micrographs
- EDX Energy dispersive x-ray spectroscopy
- a glass-crystalline particle including a glass component (glass No. 1 from Table 1) without any crystalline components wherein the glass component contains Al 2 O 3 , B 2 O 3 , Bi 2 O 3 , Li 2 O, Na 2 O, SiO 2 , TiO 2 , and ZrO 2 was prepared.
- bismuth containing solution was prepared by the dissolution of Bi(OH) 3 in 923 g of nitric acid at 50° C. After the dissolution was complete, 1000 g of deionized water was added along with 5.1 g of Al(NO 3 ) 3 .9H 2 O, 17.3 g of LiNO 3 , and 11.2 g of NaNO 3 .
- the bismuth containing solution was then added to 2695 g of deionized water and 12.0 g of colloidal ZrO 2 , 36.7 g of colloidal TiO 2 , and 54.8 g of fumed SiO 2 were added to make the precursor solution.
- the precursor solution components are described in Table 2, and the properties are described in Table 3.
- An aerosol was then generated using air as the carrier gas flowing at 45 liters per minute and an ultrasonic generator with 36 ultrasonic transducers operating at 1.6 MHz. This aerosol was then sent through an impactor to remove oversized droplets and then sent into a 3 inch diameter, horizontal quartz tube located in a 3-zone furnace with a heated length of 36 inches. The 3 zones in the furnace were set at 1000° C.
- the aerosol temperature was quenched with air and the spherical glass-crystalline particles comprising a glass component that includes Al 2 O 3 , B 2 O 3 , Bi 2 O 3 , Li 2 O, Na 2 O, SiO 2 , TiO 2 , and ZrO 2 was collected.
- SEM indicated that the glass particles were spherical and the XRD indicated an amorphous glass.
- This powder had a low surface area (SA) of 1.13 m 2 /g and low ratios of surface area to particle size: SA/d 10 of 2.17, SA/D 50 of 1.33 and SA/D 95 of 0.50.
- a spherical glass-crystalline particle including a glass component (glass No. 2 from Table 1) and crystalline components wherein the crystalline components were ZnO and Zn 2 SiO 4 and the glass component contains Al 2 O 3 , B 2 O 3 , Bi 2 O 3 , Li 2 O, Na 2 O, SiO 2 , TiO 2 , ZnO, and ZrO 2 was prepared.
- a bismuth containing solution was prepared by the dissolution of Bi(OH) 3 in 739 g of nitric acid at 50° C.
- the aerosol temperature was quenched with air and the spherical glass-crystalline particles comprising a glass component that includes Al 2 O 3 , B 2 O 3 , Bi 2 O 3 , Li 2 O, Na 2 O, SiO 2 , TiO 2 , ZnO, and ZrO 2 and crystalline components that includes ZnO and Zn 2 SiO 4 was collected.
- SEM indicated that the glass particles with the crystalline components were spherical and the XRD indicated the presence of crystalline ZnO and crystalline Zn 2 SiO 4 .
- BS-SEM revealed that the particles contained dark areas that were rich in crystalline ZnO and light areas were rich in glass.
- This powder had a low surface area (SA) of 1.03 m 2 /g and low ratios of surface area to particle size: SA/d 10 of 1.87, SA/D 50 of 1.03 and SA/D 95 of 0.38.
- SA surface area
- Examples 3 and 4 were made like Example 2 except for a change in the amount of Zn(NO 3 ) 2 .6H 2 O. Compositional details are shown in Table 2, and the physical properties are shown in Table 3. The results of SEM, BS-SEM and XRD analyses were similar to those of Example 2.
- Examples 5 and 6 were made like Example 2 except Mg(NO 3 ) 2 was used instead of Zn(NO 3 ) 2 .6H 2 O. This resulted in spherical glass-crystalline particles containing glass components of Al 2 O 3 , B 2 O 3 , Bi 2 O 3 , Li 2 O, Na 2 O, SiO 2 , TiO 2 , and crystalline components of MgO and Mg 2 SiO 4 . Results were confirmed with SEM, BS-SEM, and XRD. Compositional details are shown in Table 2, and the physical properties are shown in Table 3, below.
- Examples 7 through 9 were made like Examples 1 except that the glass-containing portions contained lead. Compositional details are shown in Table 2, and the physical properties are shown in Table 3. The results of SEM, BS-SEM and XRD analyses were similar to those of Example 1.
- Example 10 was made like Example 2 except that the glass-containing portions contained lead. Compositional details are shown in Table 2, and the physical properties are shown in Table 3. The results of SEM, BS-SEM and XRD analyses were similar to those of Example 2.
- Examples 11 through 13 were made like Example 1 except for a change in the glass composition. Compositional details are shown in Table 2, and the physical properties are shown in Table 3. The results of SEM, BS-SEM and XRD analyses were similar to those of Example 1.
- Examples 14 through 21 were made like Example 2 except for a change in the glass composition. Compositional details are shown in Table 2, and the physical properties are shown in Table 3. The results of SEM, BS-SEM and XRD analyses were similar to those of Example 2.
- Comparative glass powder samples were synthesized using methods known to those skilled in the art as conventional glass making techniques. Ingredients were weighed then mixed in the desired proportions to make a glass with the compositions listed in Table 1 and then heated in a furnace to form a melt in platinum alloy crucibles. The resulting powder properties are shown in Table 3.
- glass A (refer to Table 1) was made by heating the glass component composition to a peak temperature of 1100° C. and for a time such that the melt became entirely liquid and homogeneous. The molten glass was then quenched by pouring the molten glass directly into a room temperature bath of deionized water. The resulting glass frit or platelet was then milled to form a powder with its 50% volume distribution set between to a desired target (e.g. 0.8-1.5 micron).
- a desired target e.g. 0.8-1.5 micron
- Part of the molten glass was poured into a heated graphite mold and slow cooled to form a cast glass specimen.
- the sample was cooled by a slow enough rate to avoid residual stresses and thermal shock.
- the cast glass specimen was weighed while suspended in water to measure the glass density by the Archimede's method. Glass A had a density of 5.58 g/cc.
- the synthesized powder was analyzed by XRD to assess devitrification products and backscatter scanning electron microscopy with ED to reveal powder morphology while obtaining data about chemical composition of morphological features.
- XRD data of the bulk powder displayed characteristics of partial crystallization in a glassy matrix. Crystalline willemite, Zn 2 SiO 4 , was observed to be present with possibly some Pb phosphates.
- BS-SEM and EDX revealed that the glass A powder included particles with an irregular shaped morphology characteristic of hard glassy materials which had been milled.
- the glass A powder contained particles of two distinct types; a population of homogenous particles appearing of lighter contrast in BS-SEM with a composition of the glass component composition when analyzed by EDX, and a distinctly different population of particles appearing of darker contrast in BS-SEM with a chemical make-up of only Zn, Si, and O indicating these were particles of crystalline willemite. Some of these darker particles could be observed with some traces of a lighter contrast residue of the glassy phase on periphery of individual particles. In general, these powder samples included of primary particles of either homogenous glass or crystalline willemite. This powder had a high surface area (SA) of 8.5 m 2 /g and high ratios of surface area to particle size: SA/d 10 of 20.3, SA/D 50 of 11.7 and SA/D 95 of 3.74.
- SA surface area
- glass B (refer to Table 1) was made by heating the glass component composition to a peak temperature of 1400° C. and for a time such that the melt becomes entirely liquid and homogeneous. The molten glass was then quenched between counter rotating stainless steel rollers to form a 10-15 mil thick platelet of glass. The resulting glass frit or platelet was then milled to form a powder with its 50% volume distribution set between to a desired target (e.g. 0.8-1.5 micron).
- a desired target e.g. 0.8-1.5 micron
- Part of the molten glass was poured into a heated graphite mold and slow cooled to form a cast glass specimen.
- the sample was cooled at a slow enough rate to avoid residual stresses and thermal shock.
- the cast glass specimen was weighed while suspended in water to measure the glass density by the Archimedes's method. Glass A had a density of 4.82 g/cc.
- the synthesized powders were analyzed by XRD to assess devitrification products and BS-SEM with EDX to reveal powder morphology while obtaining data about chemical composition of morphological features.
- XRD data of the bulk powder shown in FIG. 2 displayed characteristics of partial crystallization in a glassy matrix. Crystalline willemite, Zn 2 SiO 4 , was observed to be present.
- BS-SEM and EDX revealed that the powder samples consisted of particles with an irregular shaped morphology characteristic of hard glassy materials which had been milled.
- the sample contained particles of two distinct types; a population of homogenous particles appearing of lighter contrast in BS-SEM with a composition of the glass component composition when analyzed by EDX, and a distinctly different population of particles appearing of darker contrast in BS-SEM with a chemical make-up of only Zn, Si, and O indicating these were particles of crystalline willemite. Some of these darker particles could be observed with some traces of a lighter contrast residue of the glassy phase on periphery of individual particles. In general, these powder samples included primary particles of either homogenous glass or crystalline willemite.
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4564556A (en) | 1984-09-24 | 1986-01-14 | Minnesota Mining And Manufacturing Company | Transparent non-vitreous ceramic particulate |
| JPH06211542A (ja) | 1993-01-14 | 1994-08-02 | Iwaki Glass Kk | 砥粒固定用結晶化ガラス及びそれを使用した研削砥石 |
| JPH0891874A (ja) * | 1994-09-29 | 1996-04-09 | Sumitomo Osaka Cement Co Ltd | ガラス球状粉末及びその製造方法 |
| JPH08310836A (ja) | 1995-05-11 | 1996-11-26 | Sumitomo Osaka Cement Co Ltd | ガラス球状粉末およびその製造方法 |
| JPH10194846A (ja) * | 1997-01-16 | 1998-07-28 | Sumitomo Kinzoku Electro Device:Kk | 低温焼成基板の製造方法 |
| US6000241A (en) | 1998-08-26 | 1999-12-14 | Particle Technology, Inc. | Process for making barium containing silicate glass powders |
| WO2000012437A1 (fr) | 1998-08-27 | 2000-03-09 | Superior Micropowders Llc | Poudres de verre, procedes de production de poudres de verre et dispositifs façonnes a partir de ceux-ci |
| US20010056021A1 (en) * | 2000-04-03 | 2001-12-27 | Hideki Nagata | Glass composition for crystallized glass |
| US20020007650A1 (en) | 2000-06-05 | 2002-01-24 | Murata Manufacturing Co., Ltd. | Glass powder and manufacturing method therefor |
| US7141520B2 (en) | 2001-12-12 | 2006-11-28 | Schott Ag | Antimicrobial alkali-silicate glass ceramic and the use thereof |
| US7175786B2 (en) | 2003-02-05 | 2007-02-13 | 3M Innovative Properties Co. | Methods of making Al2O3-SiO2 ceramics |
| US7258707B2 (en) | 2003-02-05 | 2007-08-21 | 3M Innovative Properties Company | AI2O3-La2O3-Y2O3-MgO ceramics, and methods of making the same |
-
2010
- 2010-09-27 WO PCT/US2010/050333 patent/WO2011038312A1/fr not_active Ceased
- 2010-09-27 US US12/891,218 patent/US8685290B2/en not_active Expired - Fee Related
- 2010-09-28 TW TW099132872A patent/TW201118048A/zh unknown
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4564556A (en) | 1984-09-24 | 1986-01-14 | Minnesota Mining And Manufacturing Company | Transparent non-vitreous ceramic particulate |
| JPH06211542A (ja) | 1993-01-14 | 1994-08-02 | Iwaki Glass Kk | 砥粒固定用結晶化ガラス及びそれを使用した研削砥石 |
| JPH0891874A (ja) * | 1994-09-29 | 1996-04-09 | Sumitomo Osaka Cement Co Ltd | ガラス球状粉末及びその製造方法 |
| JPH08310836A (ja) | 1995-05-11 | 1996-11-26 | Sumitomo Osaka Cement Co Ltd | ガラス球状粉末およびその製造方法 |
| JPH10194846A (ja) * | 1997-01-16 | 1998-07-28 | Sumitomo Kinzoku Electro Device:Kk | 低温焼成基板の製造方法 |
| US6360562B1 (en) | 1998-02-24 | 2002-03-26 | Superior Micropowders Llc | Methods for producing glass powders |
| US6866929B2 (en) | 1998-02-24 | 2005-03-15 | Cabot Corporation | Glass powders, methods for producing glass powders and devices fabricated from same |
| US6000241A (en) | 1998-08-26 | 1999-12-14 | Particle Technology, Inc. | Process for making barium containing silicate glass powders |
| WO2000012437A1 (fr) | 1998-08-27 | 2000-03-09 | Superior Micropowders Llc | Poudres de verre, procedes de production de poudres de verre et dispositifs façonnes a partir de ceux-ci |
| US20010056021A1 (en) * | 2000-04-03 | 2001-12-27 | Hideki Nagata | Glass composition for crystallized glass |
| US20020007650A1 (en) | 2000-06-05 | 2002-01-24 | Murata Manufacturing Co., Ltd. | Glass powder and manufacturing method therefor |
| US7141520B2 (en) | 2001-12-12 | 2006-11-28 | Schott Ag | Antimicrobial alkali-silicate glass ceramic and the use thereof |
| US7175786B2 (en) | 2003-02-05 | 2007-02-13 | 3M Innovative Properties Co. | Methods of making Al2O3-SiO2 ceramics |
| US7258707B2 (en) | 2003-02-05 | 2007-08-21 | 3M Innovative Properties Company | AI2O3-La2O3-Y2O3-MgO ceramics, and methods of making the same |
Non-Patent Citations (9)
| Title |
|---|
| Albarran, J. L. et al., Properties of Reinforced Glass with Crystalline Particles, Materials and Manufacturing Processes, 2006, pp. 115-119, vol. 21, Taylor & Francis LLC. |
| Cho, Jung Sang et al., Synthesis of spherical shape borate-based bioactive glass powders prepared by ultrasonic spray pyrolysis, Ceramics International, Aug. 1, 2009, pp. 2103-2109, vol. 35, No. 6, Elsevier, Amsterdam, NL. |
| Dyamant et al., Thermal properties and glass formation in the SiO2-B2O3-Bi2O3-ZnO quaternary system, Journal of Non-Crystalline Solids, pp. 3503-3507, vol. 351, No. 43-45, North-Holland Physics Publishing, Amsterdam, NL. |
| Hu, A. M. et al., Crystallization and properties of a spodumene-willemite glass ceramic, Thermochimica Acta, Oct. 15, 2005, pp. 110-113, vol. 437, No. 1-2, Elsevier Science Publishers, Amsterdam, NL. |
| Ko, You Na et al., Effect of precursor types on the characteristics of the Pb-based glass powderes prepared by spray pyrolysis, Ceramics International, Sep. 23, 2009, pp. 395-399, vol. 36, No. 1, Elsevier, Amsterdam, NL. |
| PCT International Search Report and Written Opinion, mailed Dec. 27, 2010 for co-pending U.S. Appl. No. 12/891,199. |
| PCT International Search Report and Written Opinion, mailed Dec. 27, 2010 for co-pending U.S. Appl. No. 12/891,244. |
| PCT International Search Report and Written Opinion, mailed Jan. 12, 2011. |
| Shieh, Y. N. et al., Constitution of laser melted Al2O3-Mg0-SiO-2 ceramics, Materials Science and Technology, Sep. 1995, pp. 863-869, vol. 11, No. 9, Maney Publishing, GB. |
Also Published As
| Publication number | Publication date |
|---|---|
| US20110233485A1 (en) | 2011-09-29 |
| WO2011038312A1 (fr) | 2011-03-31 |
| TW201118048A (en) | 2011-06-01 |
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